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Crystal Data for 1: C24H119N 24O79.5Cu10Ge2W18, triclinic, space group P1, Mr, 6106.12, a, 13.0014(10, b, 13.8546(11, c, 17.1074(14) Å; α, 94.6500(10)°, β, 110.1820(10)°, γ, 101.0990(10)°, V, 2801.6(4) Å3, T, 292(2) K; Z, 1, μ, 20.871 mm-1, R1, 0.0581, wR2, 0.1455 [I > 2σ(I, 14319 reflections measured, 9435 independent Rint, 0.1187, CCDC: 618905
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int = 0.1187). CCDC: 618905.
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33847647200
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Synthesis of 1: The precursor α-K8GeW 11O39 was synthesized as described in reference 11 and confirmed by IR spectrum. Other reagents were purchased commercially and used without further purification. Compound 1 was prepared from a mixture of α-K8GeW11O39, Cu(NO3)2·3H2O, KF·2H 2O, en and distilled water in the mole ratio 0.6:2:7:1.3:1100, heated in a Teflon-lined steel autoclave inside a programmable electric furnace at 160°C, for 120 h with a starting pH of 4.9, adjusted with hydrochloric acid (2 mol/L, After cooling the autoclave to room temperature for 48 h, brown crystals were obtained, filtered, washed with distilled water and dried in air. Yield: 75, C24H119N24O79.5Cu 10Ge2W18 6106.12, calcd. C, 4.72; H, 1.90; N, 5.51, Found: C, 4.38; H
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-1): 3446(s), 3259(s), 1590(m), 1458(w), 1399(m), 1110(w), 1048(m), 928(m), 908(w), 885(m), 833(w), 775(s), 715(s), 508(w), 454(w), 412(w).
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